JPH11349316A - Method for recovering suspended diamond fine particles from aqueous medium - Google Patents
Method for recovering suspended diamond fine particles from aqueous mediumInfo
- Publication number
- JPH11349316A JPH11349316A JP10192253A JP19225398A JPH11349316A JP H11349316 A JPH11349316 A JP H11349316A JP 10192253 A JP10192253 A JP 10192253A JP 19225398 A JP19225398 A JP 19225398A JP H11349316 A JPH11349316 A JP H11349316A
- Authority
- JP
- Japan
- Prior art keywords
- diamond
- recovering
- fine particles
- oil
- aqueous medium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
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- Carbon And Carbon Compounds (AREA)
Abstract
(57)【要約】
【目的】 本発明の主な目的は、水乃至水性媒質中に懸
濁しているダイヤモンド微細粒子を、少ない経費で捕集
・回収する方法を提供することである。
【構成】 本発明の方法は、水性媒質中に懸濁している
ダイヤモンド微細粒子の表面を、この媒質中で疎水性化
処理し、続いて、水に対する相互溶解性の小さな油と接
触させて油相へ移行させることを特徴とする。
(57) [Summary] The main object of the present invention is to provide a method for collecting and recovering diamond fine particles suspended in water or an aqueous medium at low cost. The method of the present invention comprises the steps of subjecting a surface of diamond fine particles suspended in an aqueous medium to a hydrophobizing treatment in the medium, and then contacting the surface with an oil having a low mutual solubility in water. It is characterized by shifting to a phase.
Description
【０００１】[0001]
【産業上の利用分野】 本発明は、水性媒質からダイヤ
モンド粒子を回収する方法、特に、水性媒質中に懸濁し
ている微細なダイヤモンド粒子を回収する方法に関す
る。The present invention relates to a method for recovering diamond particles from an aqueous medium, and more particularly to a method for recovering fine diamond particles suspended in an aqueous medium.
【０００２】[0002]
【従来の技術】 精密加工の進歩に伴い、研磨材として
用いられるダイヤモンド粉末のサイズが、サブミクロン
の細かな領域へ移行しつつある。このような微粉末は、
粗い砥粒の粉砕、整粒工程によって製造される場合が多
く、製造段階で各種の薬品処理を経る結果、粉末表面が
しばしば親水性になっている。このような粒子は水中に
懸濁し易いので、捕集が困難である。2. Description of the Related Art With the advance of precision processing, the size of diamond powder used as an abrasive is shifting to a submicron range. Such fine powder,
In many cases, the powder surface is manufactured by a process of grinding and sizing coarse abrasive particles, and as a result of undergoing various chemical treatments in the manufacturing stage, the powder surface is often hydrophilic. Such particles are easy to suspend in water and therefore difficult to collect.
【０００３】一方ダイヤモンド砥粒を用いた研磨、研削
加工において、研削屑に混じって排出される微細なダイ
ヤモンドの破片は、今まで有効な回収方法がなく、排水
と共に廃棄されているのが現状である。[0003] On the other hand, in the polishing and grinding processing using diamond abrasive grains, fine diamond fragments discharged together with grinding dust have not been effectively recovered until now, and are currently discarded together with drainage. is there.
【０００４】これらの微粉ダイヤモンドの捕集方法とし
ては、超高速遠心分離機の利用や、酸性水溶液中での沈
降（ζ電位が正になる条件下での凝集）方法が知られて
いるが、設備コストや所要設置面積が大きいことから、
現実的な解決策とは言えない。As a method for collecting these fine diamond particles, use of an ultra-high-speed centrifugal separator and sedimentation in an acidic aqueous solution (aggregation under conditions where the ζ potential becomes positive) are known. Because of the large equipment costs and required installation area,
It is not a realistic solution.
【０００５】[0005]
【発明が解決しようとする課題】 本発明は、上記の問
題に鑑み、水乃至水性媒質中に懸濁しているダイヤモン
ド微細粒子を、少ない経費で捕集・回収する方法を提供
するものである。SUMMARY OF THE INVENTION In view of the above problems, the present invention provides a method for collecting and recovering diamond fine particles suspended in water or an aqueous medium at a low cost.
【０００６】[0006]
【課題を解決するための手段】 本発明の方法は、水性
媒質中に懸濁しているダイヤモンド微細粒子の表面を、
この媒質中で疎水性化処理し、続いて、水に対する相互
溶解性の小さな油と接触させて油相へ移行させることを
特徴とする。According to the method of the present invention, the surface of diamond fine particles suspended in an aqueous medium is removed.
Hydrophobizing treatment in this medium is followed by contact with an oil having a low mutual solubility in water to transfer to an oil phase.
【０００７】本発明においては、まずダイヤモンド粒子
の表面の疎水性化を行う。このために、水性媒質に陽イ
オン性界面活性剤の添加によって行う。界面活性剤とし
ては、４級アミン、例えばｎ−ドデシルトリメチルアン
モニウムクロリド（ＤＴＡＣ）を好適な例として挙げる
ことができる。添加量は懸濁水に対して１〜５００ｐｐ
ｍ程度で充分である。In the present invention, first, the surface of diamond particles is made hydrophobic. For this, it is carried out by adding a cationic surfactant to the aqueous medium. Preferred examples of the surfactant include a quaternary amine such as n-dodecyltrimethylammonium chloride (DTAC). The addition amount is 1 to 500 pp with respect to the suspension water.
m is sufficient.
【０００８】次いでこの表面を疎水性化したダイヤモン
ド粒子を油と接触させ、ダイヤモンドを水相から油相へ
移す。この際接触頻度を高めるためには、油をエマルジ
ョン化することが必要であるが、特に振とう、攪拌、空
気の吹込みによって、油滴をできるだけ細かくするのが
好ましい。例えば浮遊選鉱分離の技術を応用して細かな
空気の泡を形成させたり、攪拌機を用いた機械的な撹
拌、超音波振動を利用した混合、反応系全体の振とう等
の手段が利用できる。Next, the diamond particles whose surfaces have been made hydrophobic are brought into contact with oil, and the diamond is transferred from the aqueous phase to the oil phase. At this time, in order to increase the contact frequency, it is necessary to emulsify the oil, but it is preferable to make the oil droplets as fine as possible, particularly by shaking, stirring, and blowing air. For example, means such as forming fine air bubbles by applying a flotation separation technique, mechanical stirring using a stirrer, mixing using ultrasonic vibration, and shaking the entire reaction system can be used.
【０００９】ダイヤモンドを濃縮するための油として
は、水との相互溶解度が小さいことが要件である。この
意味で２，２，４−トリメチルペンタン（イソオクタン
−ガソリンの主成分）や、灯油、軽油、ケロシン等の炭
化水素系の、極性の低い軽質油は好適な例であり、これ
らは入手も容易である。なお環境保全や毒性の観点か
ら、芳香族の油は避けるべきである。[0009] The oil for concentrating diamond is required to have low mutual solubility with water. In this sense, 2,2,4-trimethylpentane (a main component of isooctane-gasoline) and hydrocarbon-based light oils of low polarity such as kerosene, gas oil, and kerosene are preferable examples, and these are easily available. It is. From the viewpoint of environmental protection and toxicity, aromatic oils should be avoided.
【００１０】油の量は、添加すべき水の量に対して５％
以下でよく、通常の操業においては２％以下で十分であ
る。The amount of oil is 5% based on the amount of water to be added.
Below, 2% or less is sufficient for normal operation.
【００１１】接触によってダイヤモンドが濃縮された油
相は、蒸留によって油を回収し、蒸留残滓を洗浄してダ
イヤモンドを回収する。The oil phase in which the diamond is concentrated by the contact recovers the oil by distillation, and cleans the distillation residue to recover the diamond.
【００１２】なお、研磨、研削加工工程の排出液からの
ダイヤモンド回収に際しては、研削屑のセラミックスや
金属を分離する工程が加わることは言うまでもない。研
削屑が酸化物系の場合には浮遊選鉱法による分離が有効
であり、金属系の場合には化学薬品処理工程が付加され
る。Needless to say, a step of separating ceramics and metal as grinding waste is added to the recovery of diamond from the effluent in the polishing and grinding steps. If the grinding waste is oxide-based, separation by flotation is effective, and if it is metal-based, a chemical treatment step is added.
【００１３】[0013]
【実施例１】 浮遊選鉱分離用のカラムを用いて、懸濁
液からのダイヤモンドの回収を行った。カラムは内径４
６ｍｍ、長さ１６０ｍｍのガラス管の一端に、Ｎｏ．５
ガラスフィルタを接着したもので、これを縦型に配置し
た。Example 1 Diamond was recovered from a suspension using a column for flotation separation. Column has an inner diameter of 4
No. was placed on one end of a glass tube having a length of 6 mm and a length of 160 mm. 5
A glass filter was bonded, and this was arranged vertically.
【００１４】一方、平均粒径０．４４μｍのダイヤモン
ド粒子を４０ｐｐｍ含む２５０ｍｌの懸濁液に、陽イオ
ン性界面活性剤としてｎ−ドデシルトリメチルアンモニ
ウムクロリド（ＤＴＡＣ）の所定量を、また油として
２，２，４−トリメチルペンタン（イソオクタン）の所
定量を添加した処理水を作製し、上記カラムに入れた。On the other hand, a predetermined amount of n-dodecyltrimethylammonium chloride (DTAC) as a cationic surfactant and 2,2 as an oil were added to 250 ml of a suspension containing 40 ppm of diamond particles having an average particle diameter of 0.44 μm. Treated water to which a predetermined amount of 2,4-trimethylpentane (isooctane) was added was prepared and placed in the column.
【００１５】ガラスフィルタの底から毎分５０ｍｌの流
量で空気を吹き込み、直径数十μｍの泡で構成されたエ
マルジョンを形成し、カラムの上部から溢れ出た泡を捕
集した。泡状で捕集した液中に含まれていたダイヤモン
ド量を、使用ＤＴＡＣ濃度の関数として図１に示す。図
に見られるように、処理水１リットル当たりのＤＴＡＣ
濃度１０−２．８ｍｏｌ、イソオクタン濃度０．５６ｍ
ａｓｓ％において、約１０２０ｐｐｍ即ち約２５倍にダ
イヤモンドが濃縮された液が得られた。Air was blown from the bottom of the glass filter at a flow rate of 50 ml / min to form an emulsion composed of bubbles having a diameter of several tens of μm, and the bubbles overflowing from the top of the column were collected. The amount of diamond contained in the liquid collected as a foam is shown in FIG. 1 as a function of the DTAC concentration used. As can be seen, DTAC per liter of treated water
Concentration 10-2.8 mol, isooctane concentration 0.56m
In ass%, a solution in which diamond was concentrated at about 1020 ppm, that is, about 25 times, was obtained.
【００１６】[0016]
【実施例２】 平均粒径０．１１ミクロンのダイヤモン
ド粒子を４９ｐｐｍ含有する処理水に、イソオクタンを
１．３７ｍａｓｓ％加え、さらにＤＴＡＣを添加して液
−液抽出を行った。抽出には分液漏斗を用い、６０分間
振とうした後、２７０分間静置し、油相中のダイヤモン
ド濃度を測定したところ、ＤＴＡＣ濃度５ｘ１０−５ｍ
ｏｌにおいて約１５００ｐｐｍ（３０倍濃縮）、５ｘ１
０−６ｍｏｌにおいて約１７００ｐｐｍ（３５倍濃縮）
の結果を得た。Example 2 To treated water containing 49 ppm of diamond particles having an average particle diameter of 0.11 μm, 1.37 mass% of isooctane was added, and DTAC was further added to perform liquid-liquid extraction. A separatory funnel was used for extraction, shaken for 60 minutes, allowed to stand for 270 minutes, and measured the diamond concentration in the oil phase. The DTAC concentration was 5 × 10 −5 m.
ol about 1500 ppm (concentration 30 times), 5 × 1
In 0 -6 mol to about 1700 ppm (35-fold concentrated)
Was obtained.
【００１７】[0017]
【効果】 本発明によれば、従来研磨液と共に排出され
ていたサブミクロン級のダイヤモンド微細粒子を、簡単
な作業で有効に回収でき、再利用に供することができる
ものである。According to the present invention, submicron diamond fine particles conventionally discharged together with a polishing liquid can be effectively recovered by a simple operation and can be reused.
【図１】使用ＤＴＡＣ濃度との関数として示した、捕集
浮遊生成物（泡）中のダイヤモンド含有量FIG. 1: Diamond content in collected suspended products (foam) as a function of DTAC concentration used
───────────────────────────────────────────────────── フロントページの続き (72)発明者 日下 英史 大阪府大阪市天王寺区北山町９−40−403 ──────────────────────────────────────────────────の Continued on the front page (72) Inventor Hidefumi Kusaka 9-40-403 Kitayamacho, Tennoji-ku, Osaka-shi, Osaka
Claims (7)
微細粒子の表面を、この媒質中で疎水性化処理し、続い
て、或いは同時に、水に対する相互溶解性の小さな油と
接触させて油相へ移行させることを特徴とする、水性媒
質から懸濁ダイヤモンド微細粒子を回収する方法。1. The surface of diamond fine particles suspended in an aqueous medium is subjected to a hydrophobizing treatment in this medium and subsequently or simultaneously brought into contact with an oil having a low mutual solubility in water to form an oil phase. And recovering suspended diamond fine particles from the aqueous medium.
性剤との接触により行う、請求項１に記載の、ダイヤモ
ンド微細粒子を回収する方法。2. The method for recovering fine diamond particles according to claim 1, wherein the hydrophobizing treatment is performed by contact with a cationic surfactant.
第２級、第３級及び第４級アミン塩、並びにアンモニウ
ム塩から選ばれる一を含有する、請求項２に記載の、ダ
イヤモンド微細粒子を回収する方法。3. The method according to claim 1, wherein the cationic surfactant is a primary,
The method for recovering fine diamond particles according to claim 2, wherein the method comprises one selected from secondary, tertiary and quaternary amine salts, and ammonium salt.
と水の混合物中で行う、請求項１に記載のダイヤモンド
微細粒子を回収する方法。4. The method for recovering fine diamond particles according to claim 1, wherein the contact with the oil is performed in a mixture of the emulsified oil and water.
吹き込みによって上記エマルジョン化を行う、請求項４
に記載のダイヤモンド微細粒子を回収する方法。5. The emulsification according to claim 4, wherein the emulsification is performed by mechanical stirring, shaking, or blowing air gas.
3. The method for recovering diamond fine particles according to 1.).
である、請求項４に記載の、ダイヤモンド微細粒子を回
収する方法。6. The method according to claim 1, wherein the oil is a hydrocarbon CmHn having m> = 6.
The method for recovering diamond fine particles according to claim 4, wherein
軽油から選ばれる一である、請求項６に記載の、ダイヤ
モンド微細粒子を回収する方法。7. The method according to claim 1, wherein the hydrocarbon is gasoline, kerosene,
The method for recovering diamond fine particles according to claim 6, which is one selected from light oil.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10192253A JPH11349316A (en) | 1998-06-04 | 1998-06-04 | Method for recovering suspended diamond fine particles from aqueous medium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10192253A JPH11349316A (en) | 1998-06-04 | 1998-06-04 | Method for recovering suspended diamond fine particles from aqueous medium |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH11349316A true JPH11349316A (en) | 1999-12-21 |
Family
ID=16288223
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10192253A Pending JPH11349316A (en) | 1998-06-04 | 1998-06-04 | Method for recovering suspended diamond fine particles from aqueous medium |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH11349316A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004085030A1 (en) * | 2003-03-27 | 2004-10-07 | Japan Science And Technology Agency | Method of concentrating fine particle dispersion and method of recovering fine particle |
| JP2013056805A (en) * | 2011-09-08 | 2013-03-28 | Vision Development Co Ltd | Magnetic diamond microparticle and method for producing the same |
| JP2017128482A (en) * | 2016-01-21 | 2017-07-27 | 株式会社ダイセル | Surface-modified nanodiamond and nanodiamond dispersion |
-
1998
- 1998-06-04 JP JP10192253A patent/JPH11349316A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004085030A1 (en) * | 2003-03-27 | 2004-10-07 | Japan Science And Technology Agency | Method of concentrating fine particle dispersion and method of recovering fine particle |
| CN100415342C (en) * | 2003-03-27 | 2008-09-03 | 独立行政法人科学技术振兴机构 | Method for concentrating dispersion containing fine particles and method for recovering fine particles |
| JP2013056805A (en) * | 2011-09-08 | 2013-03-28 | Vision Development Co Ltd | Magnetic diamond microparticle and method for producing the same |
| JP2017128482A (en) * | 2016-01-21 | 2017-07-27 | 株式会社ダイセル | Surface-modified nanodiamond and nanodiamond dispersion |
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